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In this Section of the journal, the literature on continuous flow synthesis (primarily organic synthesis and functional materials) from the period of October — December 2016 is presented. All the publications are listed ordered by journal name, with two Review articles appearing at the end. In this quarter the number of papers on continuous flow organic synthesis is relatively less as a few special issues are planned in the coming months. Two contributions on machine learning for optimization in flow synthesis and the scale-up of continuous flow reactors from Eli Lilly are the real highlights of this quarter!

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Thermal decomposition of metal uranyl acetates is one of the best ways of preparation of uranates in crystalline form at low temperatures. Acetates of the type M(UO2)2(OAc)6·7H2O (M=Zn(II), Mg(II) and Ni(II) were prepared and characterised. Their X-ray powder diffraction analysis showed that they all belong to the orthorhombic crystal class.

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A Global Positioning System (GPS) permanent station has been established as a reference point at the Department of Civil Engineering of Indian Institute of Technology Bombay (IITB), by the IITB GPS group, and is continuously operating since January 2002. The station is being operated under a research project funded by the Department of Science and Technology (DST), Government of India, under the “National GPS Programme for Earthquake Studies”. A brief description of the station set up, the strategy used in determining its precise position, and some sample results are presented in this paper.

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Abstract  

Studies on bioaccessibility of elements were carried out by in-vitro gastrointestinal digestion simulation method combined with neutron activation analysis (NAA) using NH4HCO3 as an alternate base to commonly used base of NaHCO3. The effect of two bases namely NaHCO3 and NH4HCO3 on the bioaccessibility of the elements namely Br, Fe, K, La, Na, Rb, Sm and Zn from wheat seeds, fresh wheatgrass and commercial wheatgrass tablet was investigated. The bioaccessible concentrations of the elements were determined by neutron activation analysis (NAA). The bioaccessible concentrations of samples digested using NH4HCO3 were found to be higher by 10–15% for most of the elements than that observed using NaHCO3. In the case of fresh wheatgrass, the differences were as high as 50%. The present study indicated that NH4HCO3 can be used as a base instead of NaHCO3 in in-vitro gastrointestinal digestion simulation method.

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A systematic TG/DTG/DTA analysis is reported of anhydrous and heptahydrate forms of tris-phenanthroline and tris-pyridyl complexes of nickel(II), whose kinetic parameters were calculated by five different methods. The dehydration and de-ligation steps are descrete in Ni(phen)3Cl2 · 7 H2O, while those in Ni(bipy)3Cl2 · 7 H2O are mixed. Partial loss of the ligand is common for both hydrated and anhydrous compounds. In most cases the activation energyE a calculated from the mechanism-non-invoking equation of Horowitz and Metzger is in good agreement with that found from the mechanism-based relation of Mampel. There is an appreciable variation in magnitude in the results obtained from the different relations for the evaluation ofE a. It is inferred that such kinetic data are of significance in comparisons of the decomposition processes in related systems but not as absolute quantities.

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Journal of Thermal Analysis and Calorimetry
Authors: D. Bhosale, N. Choudhari, S. Sawant, V. Patil, P. Kulkarni, and V. Kelkar

Abstract  

Homogeneous solid solution oxalates of Fe2+, Cu2+, Mg2+ and Zn2+ metals were prepared by co-precipitation from respective metal acetate solutions with oxalic acid solution. The thermogravimetric (TG) analysis of co-precipitated oxalate complexes with general formula MgxCu(0.50-x)Zn0.50Fe2(C2O4)3nH2O (x=0.00, 0.05, 0.10, 0.15, 0.20, 0.25, 0.30, 0.35, 0.40, 0.45, 0.50) were carried out by manual method in static air atmosphere. The total mass loss % and stepwise mass loss % values are in good agreement with theoretically calculated mass loss % values. The thermal decomposition of oxalate complexes occur at relatively lower temperatures (561 to 698 K). The lowering of decomposition temperatures may be attributed to earlier initiation of Fe2+ oxalate in oxalate complexes. At temperatures between 598–698 K the thermal decomposition of Cu-Mg-Zn-Fe solid solution oxalate complexes leads to formation of ferrites of spinel structure. After tampering at 873 and 1273 K, homogeneous ferrites arise, which is revealed from XRD studies.

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Journal of Thermal Analysis and Calorimetry
Authors: S. R. Yoganarasimhan, N. S. Bankar, S. B. Kulkarni, and R. G. Sarawadekar

The kinetics of oxidation of metallic fuels by metal oxides involve some of the most important parameters determining the utility of any metal oxide system in pyrotechnic applications. An attempt has been made to study the oxidation of Ta metal by strong oxidizers such as PbO2 and Pb3O4, employing differential thermal analysis and infrared spectroscopy. The rate of oxidation of Ta increases with increasing oxidizer content in both Ta-PbO2 and Ta-Pb3O4, systems. A tentative mechanism for the observed phenomenon is proposed.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: Sharayu Kasar, Sumit Kumar, Aishwarya Kar, K. Krishnan, N. Kulkarni, and B. Tomar

Abstract  

Sorption of Eu(III), an analogue of trivalent actinides (Am, Cm), by amorphous titania as well as different crystalline phases of titania, namely anatase and rutile, have been studied as a function of pH, using 154Eu (half life = 8.8 yrs, Eγ = 123,247 keV) as a radiotracer. The objective of this study was to investigate the effect of the crystalline phase of the titania on their sorption behaviour towards the metal ion. Amorphous titania was prepared by organic route and was converted into anatase and rutile by heating at elevated temperatures based on the differential thermal analysis studies. Eu(III) sorption by all forms of titania rises sharply with the pH of the suspension, with the sorption edge shifting to higher value in the order; amorphous < anatase < rutile. However, the normalization of the sorption data to the surface area of the sorbents resulted in the overlapping of the sorption curves for amorphous and anatase phases, with the data being higher for rutle in the lower pH region, indicating the effect of the crystal phase on sorption behaviour of Eu(III).

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Journal of Radioanalytical and Nuclear Chemistry
Authors: N. Sonar, Vaishali De, V. Pardeshi, Y. Raghvendra, T. Valsala, M. Sonavane, Y. Kulkarni, and Raj Kanwar

Abstract  

99Tc is one of the long lived fission product with high fission yield. From radioactive waste management point of view it is very much essential to evaluate the concentration of technetium in the radioactive liquid waste in order to finalise the treatment process to extract/isolate it from the stream which is discharged to the environment. For the estimation of 99Tc in the radioactive liquid waste stream, extraction of the stable complex of technetium-tetraphenyl arsonium chloride (TPAC) into chloroform followed by beta counting was studied. Various parameters like pH, time of equilibration, concentration of TPAC in chloroform, use of other solvent for extraction as well as interference of various other radionuclides present in the waste were also studied. The radioactive liquid waste being handled in plant contains high concentrations of salts in the form of sodium nitrate. Hence effect of salt concentration on the percentage extraction was also evaluated. The extraction behavior does not dependent on change in the pH of the solution. Almost 99.5% extraction was observed in the pH range of 1–13.0. High concentration of salt is affecting the extraction. However, this can be taken care by diluting the radioactive waste. It takes almost 90 min time for maximum extraction. Presence of radionuclides like 137Cs, 90Sr are not interfering the extraction of 99Tc. However, 106Ru is getting slightly extracted along with 99Tc. The error due to 106Ru can be eliminated by taking gamma spectrum and deducting the activity from the total beta activity to get 99Tc activity. Nitrobenzene can be used for extraction of Tc–TPAC complex in place of chloroform.

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